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Performance optimization of dewatering of coal fine tailings using Box–

Behnken design

Article  in  Energy Sources, Part A: Recovery, Utilization and Environmental Effects · November 2017
DOI: 10.1080/15567036.2017.1405112

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 Energy Sources, Part A: Recovery, Utilization, and
Environmental Effects

ISSN: 1556-7036 (Print) 1556-7230 (Online) Journal homepage: http://www.tandfonline.com/loi/ueso20

Performance optimization of dewatering of coal

fine tailings using Box–Behnken design

Puja Hansdah, Shravan Kumar & N. R. Mandre

To cite this article: Puja Hansdah, Shravan Kumar & N. R. Mandre (2018) Performance
optimization of dewatering of coal fine tailings using Box–Behnken design, Energy
Sources, Part A: Recovery, Utilization, and Environmental Effects, 40:1, 75-80, DOI:
10.1080/15567036.2017.1405112

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 ENERGY SOURCES, PART A: RECOVERY, UTILIZATION, AND ENVIRONMENTAL EFFECTS
2018, VOL. 40, NO. 1, 75–80
https://doi.org/10.1080/15567036.2017.1405112

Performance optimization of dewatering of coal fine tailings using

Downloaded by [Indian Institute of Technology (ISM) Dhanbad], [Professor Shravan Kumar] at 21:56 19 December 2017

Box–Behnken design
Puja Hansdah, Shravan Kumar , and N. R. Mandre
Department of Fuel and Mineral Engineering, Indian Institute of Technology (Indian School of Mines), Dhanbad,
India

ABSTRACT KEYWORDS
The Box–Behnken design of experiments was employed to optimize the Box–Behnken design; coal
effect of variables on the settling performance of coal fine. Variable para- tailings; flocculant;
meters considered in the study were pulp density, pH, and flocculant modeling; settling
dosage, and their influence was discussed using 3D surface plot. The
study showed that a pulp density of 6% solid (w/w) was the most favorable
condition indicated a settling rate of 221 mm/min and pH of 7.5 and
flocculant dosage of 14.58 gpt were found to be the optimum condition.
The empirical models developed showed a correlation coefficient (between
experimental and predicted values) of 0.99 for settling rate.

Introduction
Run of mine coal undergoes operations such as crushing, screening, storage, conveying, and
processing that continuously increases the amount of fines (−500 µm) up to 20% of the total coal
produced (Parekh 2009). Beneficiation of these fine size coal fractions, dewatering and subsequent
disposal of tailings slurry, poses technological and environmental challenges to coal processing
industries worldwide (Kumar, Bhattacharya, and Mandre 2014; Sabah and Erkan 2006).
Dewatering process is known to depend largely on physicochemical properties of the particle
surface, mineral matter content, and size distribution along with particle shapes, specific gravities,
and their interaction with the aqueous environment (Rong and Hitchins 1995). Dewatering of fine
size coal fractions is also affected by surface charge and water chemistry of carrying liquid (Pillai
1997). The dewatering of coal fines is strongly dependent on the settling behavior in the aqueous
solution. However, the settling rate of such fine suspended particles, generally in a thickener, is very
low (Gladman, Usher, and Scales 2006). Coal being light material and exhibiting considerably lower
specific gravity (relative density) than minerals, the settling rate is significantly lower. Additionally,
the thickening process encounters difficulty owing to a significant change in the particle settling
behavior with an increase in the percentage of fines in a suspension and variation in the aggregation/
flocculation properties of the solid particles
The objective of a dewatering/sedimentation process is to determine the settling rate, clarity of
supernatant liquid, and the water content in the settled slurry, that is, sludge density (Wakeman and
Tarleton 2005). A number of studies have been conducted in the recent past that shows different
aspects of flocculation, settling, and dewatering studies of coal fines (Dash et al. 2011; Parekh 2009;
Rong and Hitchins 1995; Sabah and Erkan 2006).
Concha et al. (2012) reviewed the settling characteristics of solid particles and stated that the
fine particles may not settle at all or they may settle at a rate so slow as to be of no practical
benefit unless they are made to form agglomerates of flocs. If the particles are very small in size,

CONTACT Puja Hansdah pujahansdah@gmail.com Department of Fuel and Mineral Engineering, Indian Institute of
Technology (Indian School of Mines), Dhanbad 826004, India.
© 2017 Taylor & Francis Group, LLC
 76 P. HANSDAH ET AL.

the associated surface charge or zeta-potential is of great importance (Sabah and Erkan 2006).
Flocculants play an important role in affecting the surface charge on particles and help to
accelerate or reduce the rate of sedimentation by dispersion or agglomeration (Gupta and Yan
2006; Vergouw et al. 1998).
In a settling test, the optimizations of process parameters (pH, polymer dosage, pulp density, etc.)
are vital to achieve the desired settling performance. Therefore, an attempt has been made in the
Downloaded by [Indian Institute of Technology (ISM) Dhanbad], [Professor Shravan Kumar] at 21:56 19 December 2017

present study to improve the settling performance of coal fine tailings using cationic polyacrylamide
polymer, and the Box–Behnken design has been employed to evaluate the effect of variable para-
meters on the settling rate. Effect of operating parameters on the settling rate has been discussed
using 3D surface plot (Response Surface Methodology).

Material and methods

Fine coal tailing sample used in the present investigation was collected from the tailing pond of a
coking coal preparation plant located in the Jharia coalfield, India. A high molecular weight
cationic polyacrylamide polymer was supplied by “Innova Corporate India” in the flocculation
and settling studies of the sample to enhance the settling rate. Prior to flocculation tests, a
homogeneous stock solution (0.01%, w/w) of polymer was prepared using distilled water. The
flocculation studies were performed in a 1000 ml measuring cylinder of 6 mm diameter. For this
purpose, the slurry was prepared at desired solid concentration by properly mixing the coal
sample in water. The pH was then adjusted by using dilute Hydrochloric acid and sodium
hydroxide. Then, a desired amount of polymer solution was added into the coal slurry and
thoroughly mixed by inverting the cylinder 10–12 times (Mandre and Panigrahi 1997). After a
thorough mixing of the polymer, the cylinder was allowed to stand undisturbed. The height of
the slurry and water interface as a function of time was recorded to calculate the settling rate of
the flocculated suspension. After 15 min settling time, the clear water was taken for turbidity
measurement using a turbidity meter.
The statistical analysis was conducted using “Box–Behnken design” at three factors and one
response. The statistical software “stat-Ease Design Expert v7.0.0” was used for the determination
of the coefficient of empirical equation by the regression analysis of experimental data. The effect
of the operating variables on settling rate was presented and discussed in detail using 3D surface
plot.

Results and discussion

Characterization studies
The size analysis of representative coal sample was performed at 600, 212, 150, 106, 75, and 53
µm sieve sizes. The tailing sample indicates that approximately 80% of the particles were less
than 580 µm size. Approximately 50% of the particles were less than 300 µm size. The highest
ash content was found to be 74.44% for particles less than 53 µm size. The highest carbon
content in the sample is 29.09%. The specific gravity of the sample was 1.77. Proximate analysis
indicates that the ash content of the sample is 64.09%, volatile matter 17.69%, and fixed carbon
17.03%. The result of zeta potential study indicated that the tailing exhibits negative charge at all
pH values from 5.5 to 9.5 with no point of zero charge. A moderate zeta potential of lower
negative value of −28.79 mV at a natural pH of 7.5 of the tailing slurry in the plant indicates that
the tailing may be classified as highly stable, and stability could be disturbed by using floccula-
tion to enhance the settling characteristics. The X-ray diffraction (XRD) analysis showed that the
major minerals present in the coal sample are Quartz, illite-Montmorillonite, and kaolinite-
Montmorillonite, and the minor minerals present in the coal sample are illmenite and kaolinite
as clay mineral and dolomite.
 ENERGY SOURCES, PART A: RECOVERY, UTILIZATION, AND ENVIRONMENTAL EFFECTS 77

Statistical analysis for settling rate

Statistical design of experiments is widely reported effective in the process optimization and
modeling. The Box–Behnken design is one of the experimental designs used in the development
of new process and for the optimization of their performance for good flocculation in terms of
settling rate. To obtain the response pattern and then to establish a model, a Box–Behnken design
Downloaded by [Indian Institute of Technology (ISM) Dhanbad], [Professor Shravan Kumar] at 21:56 19 December 2017

with three factors was used. In the present investigation, three operating variable parameters are
flocculant dosage (X1), pulp density (X2), and pH (X3), as independent variables. The actual and the
coded values are presented in Table 1.
The general form of the design chosen is represented as follows:

Y ¼bo þ b1 X1 þ b2 X2 þ b3 X3 þ b12 X1 X2 þ b13 X1 X3 þ b23 X2 X3 þ b11 X1 2

(1)
þ b22 X2 2 þ b33 X3 2
where Y = the predicted response function (settling rate), bo = constant, b1,b2,b3 = linear coefficient,
b12,b13,b23 = cross product coefficient, b11,b22,b33 = quadratic coefficient, X1,X2,X3 = coded value, and
A,B,C = actual value
Totally, 15 experimental runs were conducted as per the Box–Behnken experimental design. The
experiments were performed at three levels. The Box–Behnken design with factor value in the coded
form is presented in Table 2.
For design of experiment, the result was inserted in design Expert v7.0.0 statistical software, that
is, the Box–Behnken design to obtain the response as a function of flocculant dosage, gpt, pulp
density (w/w), and pH. The regression model equation generated using these three factors and their
interaction are given in Eq. (2). The obtained regression equation in terms of actual variables is

Settling Rate ¼ 239 þ 30:96A  7:2B  25:4C þ 3:14C2  0:489AB  1:793AC  1:73BC
(2)
 0:380A2  0:235B2 þ 3:14C2
The analysis of variance (ANOVA) showing the relative significance of variable parameters and
their interaction effects on settling rate value has been shown graphically in Figure 1. Thus, it may

Table 1. Actual and coded values of the variable.

S.No Operating parameters Actual values Coded values
1. Flocculant dosage, gpt A X1
2. Pulp density,% solid (w/w) B X2
3. pH C X3

Table 2. Experiment runs for the Box–Behnken design with factor value in coded form.
Experiment Run Flocculant Dosage, Pulp density(w/ pH Actual Settling rate, Predicted Settling
number gpt (X1) w) (X2) (X3) mm/min rate, mm/min
1 0 1 −1 100.96 102.83
2 0 0 0 144.82 144.98
3 1 0 1 155.55 151.05
4 0 0 0 144.82 144.98
5 1 0 −1 192.00 187.62
6 0 −1 −1 212.12 210.66
7 1 −1 0 221.00 227.39
8 1 1 0 100.00 103.13
9 −1 0 1 103.40 108.09
10 0 0 0 144.82 144.98
11 0 −1 1 200.00 198.44
12 −1 −1 0 160.30 157.49
13 −1 1 0 58.33 52.24
14 −1 0 −1 105.00 109.8
15 0 1 1 75.00 76.77
 78 P. HANSDAH ET AL.
Downloaded by [Indian Institute of Technology (ISM) Dhanbad], [Professor Shravan Kumar] at 21:56 19 December 2017

Figure 1. Significance of variable parameteres for settling rate.

be predicted that pulp density is the most effective parameter followed by flocculant dose and pH.
However, pulp density and pH negatively affect the settling rate, and flocculant dose increases the
settling rate to increase in the dosing rate.

Effect of flocculant dosage, pulp density, and pH

Flocculation studies were conducted at a pH of 6.5, 7.5, and 8.5 at a pulp density of 6%, 8%, and 10%
solid (w/w) and with a flocculant dosage varying from 4.86 to 14.58 gpt. The effects of various operating
parameters of the settling rate are presented in Figure 2 (a, b, c). The 3D response surface plot
(Figure 2a) indicates that with an increase in the pH and increase in flocculant dosage, the settling
rate increases owing to the sufficient polymer adsorption on the particle; therefore, more suspended
particles participate in flocculation hence resulting in good settling rate. Consequently, at higher dosage
of flocculant addition, the settling rate increases owing to increase in the floc size. From (Figure 2b), it
was also observed that at a lower pulp density and increase in pH the settling rate increases. From
(Figure 2c), it was observed that with the decrease in flocculant dosage and increase in pulp density the
settling rate decreases to as low as 58.30 mm/min owing to hindered settling. At low dosages, the floc
size might be very small because of the insufficient polymer adsorption on the particles resulting in the
lower settling rate. From the study, a highest settling rate of 221 mm/min was obtained at a pH of 7.5 at
a flocculant dosage of 14.58 gpt at 6% pulp density.

Experimental versus predicted settling rate

From Figure 3, it shows that the experimental settling rates varied between 58.33 mm/min and
221 mm/min, and the predicted settling rate varied between 52.24 mm/min and 227.39 mm/
min. It shows a reasonably good agreement between the actual value and the predicted value of
the model. The correlation coefficient between actual and predicted value of settling rate was
found to be 0.99.
 ENERGY SOURCES, PART A: RECOVERY, UTILIZATION, AND ENVIRONMENTAL EFFECTS 79
Downloaded by [Indian Institute of Technology (ISM) Dhanbad], [Professor Shravan Kumar] at 21:56 19 December 2017

Figure 2. (a). Effect of flocculant dosage and pH on settling rate. (b). Effect of pulp density and pH on settling rate. (c). Effect of
flocculant dosage and pulp density on settling rate.

Figure 3. Comparison of actual and predicted settling rates.

 80 P. HANSDAH ET AL.

Conclusions
The Box–Behnken statistical experimental design method was found to be appropriate for modeling
the effects of important variable parameters of the settling rate. The prediction of response function
determined by regression analysis was in good agreement with the experiment results. Pulp density is
the most effective parameter followed by flocculant dose and pH. However, pulp density and pH
Downloaded by [Indian Institute of Technology (ISM) Dhanbad], [Professor Shravan Kumar] at 21:56 19 December 2017

negatively affect the settling rate, and the flocculant dose increases the settling rate to increase in the
dosing rate. The R2 values between the experimental and the predicted values of the settling rate
were found to be 0.99 indicating a good agreement between them. The highest settling rate of
221 mm/min was obtained at a pH of 7.5 at a flocculant dosage of 14.58 gpt at 6% pulp density.

ORCID
Shravan Kumar http://orcid.org/0000-0003-1510-4147

References
Concha, A. C., N. N. Rulyoy, and J. S. Laskowski. 2012. Settling velocities of particulate systems 18: Solid flux density
determination by ultra-flocculation. International Journal of Mineral Processing 104–105:53–57. doi:10.1016/j.
minpro.2011.12.007.
Dash, M., R. K. Dwari, S. K. Biswal, P. S. R. Reddy, P. Chattopadhyay, and B. K. Mishra. 2011. Studies on the effect of
flocculant adsorption on the dewatering of iron ore Tailings. Chemical Engineering Journal 173:318–325.
doi:10.1016/j.cej.2011.07.034.
Gladman, B. J., S. P. Usher, and P. J. Scales. 2006. Understanding of thickening process, keynote address. Australian
Centre for Geomechanics, Perth. ISBN 0-9756756. 5–6.
Gupta, A., and D. S. Yan. 2006. Introduction to mineral processing design and operation, 1st ed.Elsevier.
Kumar, S., S. Bhattacharya, and N. R. Mandre. 2014. Characterization and flocculation studies of fine coal tailings.
Journal of the Southern African Institute of Mining and Metallurgy 114:945–49.
Mandre, N. R., and D. Panigrahi. 1997. Studies on selective flocculation of complex sulphides using cellulose xanthate.
International Journal of Mineral Processing 50:177–86. doi:10.1016/S0301-7516(97)00013-6.
Parekh, B. K. 2009. Dewatering of fine coal and refuse slurries problems and possibilities. Procedia Earth and Planetary
Science 1:621–26. doi:10.1016/j.proeps.2009.09.098.
Pillai, J. 1997. Flocculants and Coagulants: The Keys to Water and Waste Management in Aggregate Production.
Condensed version appeared in December issue of Stone Review, Nalco Company.
Rong, R. X., and J. Hitchins. 1995. Preliminary Study of Correlations between Fine Coal Characteristics and Properties
and their Dewatering behavior. Mineral Engineering 3:293–309. doi:10.1016/0892-6875(94)00126-W.
Sabah, E., and Z. E. Erkan. 2006. Interaction mechanism of flocculants with coal waste slurry. Fuel 85:350–59.
doi:10.1016/j.fuel.2005.06.005.
Vergouw, J. M., A. Difeo, Z. Xu, and J. A. Finch. 1998. An aglomeration study of sulphide minerals using zeta-
potential and settling rate, Part I: Pyrite and galena. Mineral Engineering 2:159–69. doi:10.1016/S0892-6875(97)
00148-9.
Wakeman, R. J., and E. S. Tarleton. 2005. Scale up of industrial equipment. In Solid-liquid sepration, 1st ed., 4–7.
Elsevier.

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